同位素内标-液相色谱串联质谱法测定动物源食品中的脱氢胆酸  

Determination of dehydrocholic acid in animal-derived food by isotopic internal standards-liquid chromatography-tandem mass spectrometry

作　　者：吴社莲 袁列江 李政 吴海智 徐文泱 WU Sheian;YUAN Liejiang;LI Zheng;WU Haizhi;XU Wenyang(Hunan Provincial Product Evaluation Center,Changsha 410018;Hunan Institute of Product and Goods Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410017)

机构地区：[1]湖南省产商品评审中心,长沙410018 [2]湖南省产商品质量检验研究院,食品安全监测与预警湖南省重点实验室,长沙410017

出　　处：《中国食品添加剂》2024年第12期186-196,共11页China Food Additives

基　　金：国家市场监督管理总局研究委托任务;湖南省自然科学基金(2022JJ90007,2022JJ90029)。

摘　　要：脱氢胆酸在我国是一种未列入兽药名单的利胆药,已有水产品养殖企业将其添加至饲料中以增强动物免疫力。本文建立了一种动物源性食品中脱氢胆酸的同位素内标-液相色谱串联质谱检测方法。样品经乙腈提取后以乙腈饱和的正己烷净化,采用内标法进行定性定量分析。考察了提取条件、净化方法对实验结果的影响,优化了仪器参数,并建立了方法学技术参数。结果表明,该方法在5~250 ng/mL之间线性关系良好,回收率在82.0%~110.0%之间,精密度<12%,满足方法学技术参数的相关要求。Dehydrocholic acid is a choleretic agent not listed in the veterinary drug catalog in China,and it has been added to feed by aquaculture companies to improve animal immunity.A method was developed for the determination of dehydrocholic acid in animal-origin foods using isotope internal standard liquid chromatography-tandem mass spectrometry.After extraction with acetonitrile,the samples were purified with n-hexane saturated by acetonitrile,and qualitative and quantitative analysis were carried out using an internal standard method.The effects of extraction conditions and purification methods on the experimental results were investigated,the instrumental parameters were optimized,and the technical parameters of the methodology were established.The results showed that the method had a good linear relationship between 5 and 250 ng/mL,the recovery rate was between 82.0%and 110.0%,and the precision was less than 12%,which met the relevant requirements of the methodological technical parameters.

关 键 词：同位素 液相色谱-串联质谱 脱氢胆酸 

分 类 号：TS207.3[轻工技术与工程—食品科学]